Apparatus for the regular and continuous distillation of resins.



L. B. GASTETS. APPARATUS FORTHE REGULAR AND GONTINUOUS DISTILLATION OF RESINS.

' APPLICATION PIL'B!) fun 22, 1909.

1,652,214. Patented Feb.4,.1913

I 50 A 2 SHEETS-SHEET 1.

inventor. $1M

MA. I

L. B. GASTETS. APPARATUS FOR THE REGULAR AND commuous DISTILLATION or RESINS.

, AfiPI-IOATION FILED JUNE 22, 1909. 1 952 214, Patented Feb. 4, 1913 2 SHEET S-SHEET 2.

Inventer.

' Witnesses LOUIS. BABTHELEMY CASTETS, or LALUQUE, rnLNcE.

arranarus son REGULAR am) e'ourimrou's nIs'rrL A'rIoN or nnsms.

To all whom it may concerns 1 l I v Be it known that-I, LOUIS BARTHELEMY Cas'mrs,' a citizen of the Republic of France,

, and residing at Laluque, Landes, in the said,

.5 Republic, engineer, have invented certain new and useful Improvements n Apparatus for the Regular and Gontlnuous Distillation of Resins; and I do herebydeclare the fol lowing to bea full, clear, and exact description of the'inve'ntion, such as will'enable others skilled in the art to which it appertains tomake and use the same, reference being had 'to the accompanyingdrawings,

and to letters or figures of reference marked thereon, which form a part of this spccification.

the. distillation of resins and has for its object to insureacontinuity of the operation Q'QfOW'i'Hg tuthe'regular travel of .the products in a constant forward direction and to elfect a large production and a very efiicien-tout -put.

A further object 1s.to provide for the col- 26 1ecti0n of the whole of the'utilizable'essencs contained in the gums treated and a collection of the combustible gases which are not condensed, as well as of the residual liquids from distillation.

30 This apparatus consists essentially in pro viding a series of distilling columns which are subjected to the action; of a vacuum and heated by the steam which circulates through the apparatus in-thc inverse order of the progress of the distillation, sa d steain then proceeding to heat a rectifying ap-' paratus where, after dondensation'a'nd still under vaccum, a new-distillation is eifected -.ot the products which have not been distilled 40. in the preceding distillationl' The invention further consists in providing refrigerating-coils serving to condense, reith er-nnder a vacuum 'or underia'fslightl pressure, the vapors produced by the; distillation, which, whenfirst liquefied, are, as well as the residual liquids from (1istil lati0n,; collected in reservoirs provided for this -pur pose. To this distillingapparatus is adde what-is preferablytermed a preparatory al 't e paratus, in whijch the gums constituting raw material are progressively crushed and trituratedunder heat, then" dissolved-a separated from-the solid residues, so as toobtain a homogeneous liquid which, under the aetio'n-ofr'a vacuum maintained'inthe distilling I apparatus passes into the" disti-lj Specification of Letters Patent. Application filed June 22, 1909. .serial 1P0. 503,615.

Patented Eeb. 4,.1913.

-ling'columhs. An automatic governor insures the regularity of the'di'stillation by producing an automatic delivery of steam into the liquid being distilled, as soon as the vacuui Ydiminishes-in .the whole of the apparatus, so as to always reestablish the. equilibrium of the distillation,

In the accompanyi'n drawings:Figure. 1' is a diagrammatic ve evat-ion of one portion of the apparatus and Fig 1" is a like.

view of another portion thereof. Fig; 2 is a view, on a larger scale, ,of the automatic adjuster shown on Fig. -1.' i

The preparatory apparatus comprises a hopper 1,\ int0 which the'raw gum is intro-' duced and which-opens below. into a mixer The-inyention relatesto anapparatus for.

comprising an endless-conven r screw 2 rotata-hly mounted in a casing 3. The convolutions ofsaid screw diminish continuously so as to, act on 'the material with a gradua ally increasingrpressurei Surrounding the.

casing 310i screw2. is a jacket 3" through which circulates steam which enters through a pipe 4.-and-passes out through a tube-5 into thehollow axle -'6 of the screw 2 so as to con municate heat-to' the convolutions of the the mas s undergoes ii-complete filtration, so. 4 I asto flow in a-perfectly homogeneous state into a lowcr'reservoiri 9. This latter comprises aiacket 10, through; which circulates the'condens ed :steam .which'. flows from the" hollow shaft 6 'of the endlesssc'rew into a conduit 11 whence it passes into the jacket '10; the 'eiracuat-ion ofthis condensed steam occursat 12. The operation of filtration of t-he.- dissolved and triturated' upon-the:

filters? and 8, takes :place under-'exclusion.-

of air, the reservoir 9"being7cog'ered"by: a

' hood-13 :theclose joint ofwhich'fat the. base ;-is insured b -'a hydraulic "joint-14., The 5 front "extrexn t of the-.conduit-o f the endless screwis supported bya' spherical .piv'ot' 1.5

' on aisupporting column" 16, so that by .rais-v ling; hood'l'3. by means of the upper lifts: ing rings 17, thelwholejmixerrinay be caused to turn. on the .pivot'15 -in-order' to enable the cleaningof theffiltrs-to bev effected. A

' tube 18, is situated a dis ther, the escape of the condensed steam tube 18 connects the lower part of the reser-f per" part with filter 47,.above' which a pipe ;voir 9' with the distilling apparatus hereinafter described andthrough said tube the liquid, whichiscontained in the reservoir is caused to lrise by means of a vacuum, created in the distilling apparatus by the pump shown at 71, Fig. 1, as will-be also hereinafter described.

The distillation apparatus comprises two distilling columns 19 and 20. The first colulnn.19 contains an interior-series of tubes 21 heated by steam which comes from a pi e '22 and is confined for a tlme'bet-ween t e two tube plates 23 and 240i this series through w 'ch the liquid-being distilled circulates'. The column 19"has a double bottom 25, into whichthe steam after circulat-,

ing around the series of pipes 21, passes by means of a pipe 26, and escapes from said bottom into a pi e 27.- The liquid to be' d15- tilled enters at t e lower part of the column- 19' from tube 18 which is provided with a tween two plates 32 and 33, a double bottom- 34, a steam circulation pipe 35, an up er inspection opening 36 and a partition p ate 37. But at the lower from the double bottom 34 is efiect-ed through a: discharge pipe 39.

through a pipe 41 opening slightly above' the up er tube plate 32 of'column 20 and controllied by a cock, situated in the pipe 41 at 42.

The steanrwhich circulates around the series of tubes '31 enters the column 20 through aside pipe 43, and it passes from column 20 to column 19 by the pipe 22 which is provided with an expander 44. The steam admitted to the series of tubes 31 is saturated steam at-3- atmospheres, that is to say at-I34.C.; and the expander 44 expands *the steam to 1 atmosphere so that it has only. a temperature of 100 (3., when admitted'to the series 21. Beyond the second distilling column 20 is situated acolophony reservoir '45 provided at its lower end with a discharge cock 46 and -at'its upart, instead of a arge cock 38; fur-j The passage ofthc liquid under treatment from the first 41 from the column 20 enters. In the cover 48 of the reservoir 45 is arranged an 1nspection glass 49 to permit of the level ofthe liquid in this reservoir being ascertained.

In o'rderto insure the continuous operation of. the apparatus different colophony reservoirs maybe alternately placed in communication with the-column 20. The two distilling columns 19 and 20 open at thenup' per partinto a collecting tube 50 which leads to a condensing coil 51, at the entrance Branch tubes 54,55 form a continuation of the coil 51, the descending tube 54 being fitted with an inspection glass 54; it serves -for'the passage of the condensed liquid,

whilethe ascending tube 55 serves for the passage'of the vapors which have escaped condensation. The first of these branch -of which is arranged a cock 52, said coil I being situated in a refrigerating "vat 53.

tubesopens into the lower part and the latter into-the upper part of, a rectlfier 56.

of theintro notion of a certain quantity of suitable crystals, preferably consisting in part of chlorid of calcium and of soda, so as to'neutralize the spirits. It is: in this part of the apparatus that the rectification is effected by second distillation. In the tube 54, an' escape cock 59'is provided, and at 60 is arranged an automatic discharge for condensed steam, the rectifier being heated by the steam which proceeds from the first dis-, tilling column 19 by pipe 27. Asecond con-- densin coil,61, communicating by tube 62 with the rectifier-56 and immersed in the refrigeration vat 63, permits of the condensation of the spirits disengaged by the rectification. The products'of condensation pass through a tube provided with an inspection opening 64 and with a cock 65 into a spirit reservoir 66, which is provided with the two draw-off tubes having cocks 67 and 68.-

The' spirit reservoir 66, communicates through a suction ipe 69 provided with a vcock 70, with an air pump 71 of any suitable type, serving, to maintain .-a vacuum throughout thewho le apparatus. The outlet pipe 72 of this pump leadsto another condensing coil 73 into which the; gases, which have survived the preceding condensation efiected'under vacuum, are forced'at a pressure of 1- atmosphere, and are then, to

a large extent, condensed and flow out into a lower receptacle 74 provided with a safety valve 75 and a discharge cock 76. This receptacle 74 communicates bya descending tube 7 7, with a reservoir 78containing at the beginning heavy spirits, in whichthe major part of the extra-light un'condensed isfurnished with a discharge cock 79; and a spirits becoinedissolved. The reservoir safety valve 80 throu h which the uncondensable but combustible gases escape, and

are conveyed to the furnaces of steam generators (not'showny The automatic adjustment of .theapparahis is elfected by a receptacle which has two Th is arm 81 has graduations- 87 enabling fl e ifi tent of the vacuum, which exists in the apparatus, to be observed. When. the degree, ofifir'haustion in the. entire apparatus changes', the mercury IlSBSlOI' descends more ordessfiin thelarger branch of the tube 81, in consequence of which ,the float 82, ar-

ranged in the other branch, rises or falls in a corresponding ma'nneryas this rise or fall operates the valve 84, for admitting steam, the control of the latter is consequently directly produced by the degree of. vacuum in the apparatus, in such amanner that the admission of steamis increased when the vacuum decreases and is diminished when the contrary is the'case. A tube 88 places'the colophony reservoir in communication with the-collector and permits the action .of,the vacuum to be also,exercised in this reservoir.

The operation of the apparatus is as follows: The raw gum is introduced into the hopper 1 of the preparatory apparatus and is carried fouwar by the endless screw 2, in

. the casing. of which it is crushed and liquele'cts in thelower reservoir 9, whence it is fied. The liquid product is purified in its passage through the filters 7 and 8 and colraised into the distilling apparatus by suction caused by the vacuum in -the apparatus proper, the quantities raised being regulated by the opening of the supply valve 28. The air pump 71 producing the vacuum in the .apparatus, the docks 70, 65, 52 and 28 being open, the vacuum is raised until the mercury of the regutator indicates a vacuum of centimeters below atmospheric pressure on the graduation 87; then thefloat 82 will be in a position to cause the rod 83 to close the steam supply valve 84:; Steam at three'atmospheres is then introduced through pipe and after its passa e 'throughthe eX-.

to 1 atmosphere so that the column 20 willbe heated to 134 pander 4,4 it is ,lowere and the colurnh 19 as well ,asthc rectifier 56, to 100 Gt, only. Theopening ofvalve 28 spirit reservoir 66. pors, composed of light spirits and some unthen permits the melted gum contained in' reservoir 9 to. be sucked through pipe 18, enter column 19, pass through the series of tubes 21, spread itself out in a thin layer on the upper tube plate 23 and pass by tube 40 into the second column 20. In its passage through the series of tubes 21, the gum is raised to a temperature of 100 C., and a starting of the distillation will occur which involves the whole of the water contained naturally ,in' the gum, plus an appreciable quantity of the spirit of turpentine. These first vapors pass into the collector 50.1. The liquid gums passing by tube 40 into the column 20 -ascend through the series of tubes 31,

where under the temperature of 134 C.,

which is obtained there, they give up all the spirits of turpentine which they contain, and which also proceed to the collector 50. The gumlnow transformed into colophony or pitch) spreads itself out -in a thin layer on the upper tube plate 32 and passes. by tube 41 nto the colophony reservoir 45, where it is filtered and whence it is drawn oil through cook 45. The circulation of the liquid from one distilling column to the other and in the colophony reservoir is eifected by the (litterence of level which, as will be seen in the drawing, exists between these three elements. The vapors proceedingfrom the distillation in the two columns uuite'in the collector 50 .and'are condensed together in the refrigerator 51. T he condensed liquid passes through the descending tube 54" with'its inspection opening 54" into the rectifier 56, where the neutralization of the spirits and their fresh distillation is effected. The vapors produced, as well as those passing by the ascending tube 55, proceed to be condensed to getherjn the second refrigerator 61 the condensed liquid flowing outthrough the tube having theinspection opening 64, into the The uncondensed vacondensable gases, are forced out by pump 71 into refrigerating coil 73 at a pressure of '1 atmosphere above atmospheric pressure, and are condensed and flow into the reservoir 74. The extra. light spirits then pass to be broken up in heavy-spirits contained in reservoir 78, while the combustible gases escape through valve 80. In the drawing, the unfeathered arrows indicate the travel of the solid and liquid products, while the feathered arrows indicate the pathof travel of the gaseous products of distillation.

The mercury regulator, while acting as a vacuum indicator, has, as already stated, the object of maintaining the equilibrium of distillation and this without augmenting the temperature in the distillin columns. In fact if for any reason the vacuum should diminish, the column of mercury descends in the long arm of the receptacle 81, and ascends in fithe other arm and thus raises the loat- 82 which opens the steam supply valve 84-. The steam thus passing through tube 89 to the bottom of the distilling column 20.

will be injected into the mass contained therein and in this manner insure the total elimination ofthe spirits.

It is evident that instead of two distilling columns, a larger number may be employed which will always be arranged in series; the same applies to the condensing refrigerators, the number of which and their arrangement may evidently vary according to the nature of the products to be treated. In the same way the details ofconstruction of the apparatus described and shown may be modified without departing from the principle of the invention. I v

I claim Apparatus "for the regular and continuous distillation of resins, con'iprising means for the preparatory treatment; of the raw gums, a series of distilling columns gravity discharging fronr,o11e to the other and above the preparatory means, series of tubes situated in said columns and heated by steam \vhich circulates in the opposite direction to that of the distillate, a reservoir for collect- -uncondensed spirits, and heavy spirit ing the residual liquid from the distillation and connected to the vapor discharge of said columns, refrigerating coils for condensing the distilled products, a rectifier for again distilling the condensed liquid with the addition of suitable products, a series of tubes arranged in said rectifier and heated by steam, condensation coils, a reservoir for the condensed products; a pump for main-- taining a vacuum in all the iIbOVC'THOHtlOHWl apparatus and thereby causing the continuous elevation of the gums to the first ol. the

series of stills, a plurality of refrigerators to receive and condense the products forced therein under slight pressure by said pump, a reservoir for collecting the eoml rmscd product, a reservoir receiving the ex ra l ght ll) this reservoir for dissolving these ext ra light spirits.

In testimony that I claim the foregoing my invention, 1 have signed my name in presence of t\\'() subscribing witnesses.

LOUIS Bilt'llllihEillY CAS'IFETS.

\Vitnesscs A. ltnxann, J. I). \VlsE. 

